CN102005559B - Method for preparing artificial graphite cathode material for lithium ion batteries - Google Patents
Method for preparing artificial graphite cathode material for lithium ion batteries Download PDFInfo
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- CN102005559B CN102005559B CN2009100703133A CN200910070313A CN102005559B CN 102005559 B CN102005559 B CN 102005559B CN 2009100703133 A CN2009100703133 A CN 2009100703133A CN 200910070313 A CN200910070313 A CN 200910070313A CN 102005559 B CN102005559 B CN 102005559B
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000010406 cathode material Substances 0.000 title claims abstract description 8
- 229910021383 artificial graphite Inorganic materials 0.000 title claims abstract description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000000463 material Substances 0.000 claims abstract description 47
- 238000005087 graphitization Methods 0.000 claims abstract description 29
- 239000011280 coal tar Substances 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 239000004005 microsphere Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000011294 coal tar pitch Substances 0.000 claims description 13
- 239000002931 mesocarbon microbead Substances 0.000 claims description 13
- 239000011302 mesophase pitch Substances 0.000 claims description 13
- 238000012545 processing Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 240000003936 Plumbago auriculata Species 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000000703 high-speed centrifugation Methods 0.000 claims description 2
- 238000012719 thermal polymerization Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 22
- 239000012286 potassium permanganate Substances 0.000 abstract description 16
- 239000011300 coal pitch Substances 0.000 abstract description 9
- 229910002804 graphite Inorganic materials 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 8
- 239000011295 pitch Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 abstract 2
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 10
- 238000006116 polymerization reaction Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002969 artificial stone Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000013031 physical testing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for preparing an artificial graphite cathode material of lithium ion batteries and belongs to the technology of the graphite cathode material of the lithium ion batteries. The method comprises the following steps of: adding coal pitch or a mixture of the coal pitch and coal tar into a reaction kettle, polymerizing at the temperature of between 350 and 480 DEG C for 5 to 15 hours, introducing the reaction product and unreacted raw materials into a cooling groove to cool the reaction product and the unreacted raw materials in order to stop the reaction, centrifugating solid substances, namely intermediate-phase pitch microspheres with a centrifugal device, drying the intermediate-phase pitch microspheres, soaking the intermediate-phase pitch microspheres with KMnO4/toluene solution, recovering toluene at a low temperature, and graphitizing the intermediate-phase pitch microspheres soaked with KMnO4 at the temperature of 2,300 DEG C, wherein the graphitization degree is more than 89 percent. The method has the characteristics of reducing the material purity and cost of the intermediate-phase graphite microspheres, reducing the high-temperature graphitization cost and improving the market competitiveness of the intermediate-phase graphite spheres.
Description
Technical field
The present invention relates to a kind of preparation method of artificial graphite cathode material for lithium ion batteries, belong to the graphite negative material of lithium ion battery technology.
Background technology
The research of the lithium battery of China continues nearly 20 years, and along with to the improvement of current material and battery design technology and the appearance of new material, the range of application of lithium ion battery is constantly expanded.At present China has become the second-biggest-in-the-world lithium ion battery producing country that is only second to Japan, and under the metastable background of lithium-ion electric pool technology, the higher price of lithium ion battery itself just becomes the bottleneck that lithium ion battery develops.
Wherein the cost performance of lithium ion battery negative material directly affects the cost performance of lithium ion battery.The price of natural graphite material is lower, but because this defective in aspect of performances such as circulation, multiplying power, batch consistency, high low temperature of native graphite causes native graphite---comprise that modifying natural graphite and native graphite clad material are difficult to be applied in high-end lithium ion battery.And a kind of as Delanium of Graphitized MCMB has obvious performance advantage: (1) long cycle performance.Graphitized MCMB coordinates the systems such as the good positive pole of cycle performance and electrolyte, and under normal operating position, circulating still has for 2000 times the capacity more than 80% to remain; (2) high rate performance.Graphitized MCMB takes off the embedding passage because of having good graphite laminate structure and lithium ion embedding one, make Graphitized MCMB have excellent multiplying power charging and multiplying power discharging property in other materials, use Graphitized MCMB to charge under 30 times of normal charging currents as the lithium ion battery of negative pole, still can be charged to more than 80% of rated capacity; (3) high temperature performance.Delanium Graphitized MCMB surface texture is perfect, be used in conjunction with PC base electrolyte and can not produce obvious side reaction, make this coordinate lithium ion battery to use under low temperature condition, equally, due to the stability of internal structure, this material can not occur similar native graphite produce under higher temperature with electrolyte in the violent side reaction of solvent.Although the Delanium Graphitized MCMB has advantages of above-mentioned very outstanding, but due to more than the high temperature graphitization of Delanium expense generally will reach 2800 degree, so graphited expense is very high, cause the cost compare of this material high, limited the further extensive use of this material.The research discovery, the existence of some metallic element has good catalytic effect for promoting carbon structure to be further converted to graphite-structure.Simultaneously, this catalyst can gasify fast and effectively at suitable temperature and discharges.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of artificial graphite cathode material for lithium ion batteries, the method have the advantages that process is simple, production cost is low.
The present invention is realized by following technical proposals, a kind of preparation method of artificial graphite cathode material for lithium ion batteries, and described artificial plumbago negative pole material refers to that average grain diameter is 6～28 μ m granular graphites, is characterized in that comprising following process:
(1) with the mixture of coal tar pitch or coal tar pitch and coal tar, in mixture, coal tar pitch and coal tar volume ratio are to add high-temperature high-pressure reaction kettle at 2～5: 1, at 350～480 ℃, under 2～6 atmospheric pressure, thermal polymerization 5～15 hours makes the part coal tar pitch change into the mesophase pitch microballoon;
(2) the resulting mixture that contains viscoelastic phase coal tar pitch, mesophase pitch microballoon of step (1) is imported be preinstalled with in the cooling bath of this mixture room temperature coal tar of 5 times of volumes, reduce below the temperature to 300 ℃ of mixed material;
(3) step (2) gained mixture is imported centrifugation and washing in the high speed centrifugation device, the mesophase pitch microballoon is separated from other solution, and fully washed the mesophase pitch microsphere surface with solvent;
(4) the mesophase pitch microballoon that obtains with step (3) is that to be dispensed into temperature at 1: 1 be to flood in the KMnO4 of 40 ℃ and toluene mixed solution according to volume ratio, and wherein the KMnO4 mass concentration is 0.1～0.5%, and dip time is 30min;
(5) then the 150 ℃ of oven dry of mixture heating that step (4) obtained contain mesophase pitch microsphere particle thing carry out graphitization processing to remove and to reclaim toluene at the temperature of 2300 ℃, obtain the Graphitized MCMB of material degree of graphitization 89.3%.
Characteristics of the present invention are, the mixture of coal tar pitch or coal tar pitch and coal tar is as the raw material of reaction, raw material be easy to get and purity requirement low, cost easily reduces; Adopt KMnO
4As the catalyst of mesophase pitch microballoon high temperature graphitization, can reduce the temperature that Carbon Materials transforms to graphite material, guaranteeing to have reduced temperature requirement on the degree of graphitization basis of product, reduce product cost, be easy to the market expansion of Graphitized MCMB.
Embodiment
Embodiment 1 injects the HTHP polymeric kettle with medium temperature coal pitch 400mL and coal tar 100mL, and slowly heating, heat up and temperature is remained on 415 ℃ of lower 10h under stirring condition.Also stir in coal tar with 5 times of volumes of the importing of the material after polymerization reaction.When making the temperature of this system be cooled to 290 ℃, then by centrifugal separating device with Separation of Solid and Liquid.Isolated solid cleans rear 120 ℃ of dry 3h with toluene, and it is to flood in the KMnO4 of 40 ℃ and toluene mixed solution that dried solid is imported temperature according to the volume ratio ratio of 1: 1, and wherein the KMnO4 mass concentration is 0.2%, and dip time is 30min.Above-mentioned material is warmed up to 150 ℃ in drying box, oven dry is to remove and to reclaim toluene.The material that obtains is carried out graphitization processing under 2300 ℃, be the product of 16～18 μ m extracting average grain diameter, material degree of graphitization 89.7%.
Embodiment 2 injects the HTHP polymeric kettle with medium temperature coal pitch 300mL and coal tar 100mL, and slowly heating, heat up and temperature is remained on 415 ℃ of lower 10h under stirring condition.Also stir in coal tar with 5 times of volumes of the importing of the material after polymerization reaction.When making the temperature of this system be cooled to 290 ℃, then by centrifugal separating device with Separation of Solid and Liquid.Isolated solid cleans rear 120 ℃ of dry 3h with toluene, and it is to flood in the KMnO4 of 40 ℃ and toluene mixed solution that dried solid is imported temperature according to the volume ratio ratio of 1: 1, and wherein the KMnO4 mass concentration is 0.2%, and dip time is 30min.Above-mentioned material is warmed up to 150 ℃ in drying box, oven dry is to remove and to reclaim toluene.The material that obtains is carried out graphitization processing under 2300 ℃, be the product of 16～18 μ m extracting average grain diameter, material degree of graphitization 89.6%.
Embodiment 3 injects the HTHP polymeric kettle with medium temperature coal pitch 400mL, and slowly heating, heat up and temperature is remained on 430 ℃ of lower 10h under stirring condition.Also stir in coal tar with 5 times of volumes of the importing of the material after polymerization reaction.When making the temperature of this system be cooled to 290 ℃, then by centrifugal separating device with Separation of Solid and Liquid.Isolated solid cleans rear 120 ℃ of dry 3h with toluene, and it is to flood in the KMnO4 of 40 ℃ and toluene mixed solution that dried solid is imported temperature according to the volume ratio ratio of 1: 1, and wherein the KMnO4 mass concentration is 0.2%, and dip time is 30min.Above-mentioned material is warmed up to 150 ℃ in drying box, oven dry is to remove and to reclaim toluene.The material that obtains is carried out graphitization processing under 2300 ℃, be the product of 16～18 μ m extracting average grain diameter, material degree of graphitization 89.3%.
Embodiment 4 injects the HTHP polymeric kettle with medium temperature coal pitch 400mL, and slowly heating, heat up and temperature is remained on 430 ℃ of lower 12h under stirring condition.Also stir in coal tar with 5 times of volumes of the importing of the material after polymerization reaction.When making the temperature of this system be cooled to 290 ℃, then by centrifugal separating device with Separation of Solid and Liquid.Isolated solid cleans rear 120 ℃ of dry 3h with toluene, and it is to flood in the KMnO4 of 40 ℃ and toluene mixed solution that dried solid is imported temperature according to the volume ratio ratio of 1: 1, and wherein the KMnO4 mass concentration is 0.2%, and dip time is 30min.Above-mentioned material is warmed up to 150 ℃ in drying box, oven dry is to remove and to reclaim toluene.The material that obtains is carried out graphitization processing under 2300 ℃, be the product of 16～18 μ m extracting average grain diameter, material degree of graphitization 89.6%.
Embodiment 5 injects the HTHP polymeric kettle with medium temperature coal pitch 400mL, and slowly heating, heat up and temperature is remained on 430 ℃ of lower 10h under stirring condition.Also stir in coal tar with 5 times of volumes of the importing of the material after polymerization reaction.When making the temperature of this system be cooled to 290 ℃, then by centrifugal separating device with Separation of Solid and Liquid.Isolated solid cleans rear 120 ℃ of dry 3h with toluene, and it is to flood in the KMnO4 of 40 ℃ and toluene mixed solution that dried solid is imported temperature according to the volume ratio ratio of 1: 1, and wherein the KMnO4 mass concentration is 0.4%, and dip time is 30min.Above-mentioned material is warmed up to 150 ℃ in drying box, oven dry is to remove and to reclaim toluene.The material that obtains is carried out graphitization processing under 2300 ℃, be the product of 16～18 μ m extracting average grain diameter, material degree of graphitization 91.5%.
Embodiment 6 injects the HTHP polymeric kettle with medium temperature coal pitch 400mL, and slowly heating, heat up and temperature is remained on 430 ℃ of lower 10h under stirring condition.Also stir in coal tar with 5 times of volumes of the importing of the material after polymerization reaction.When making the temperature of this system be cooled to 290 ℃, then by centrifugal separating device with Separation of Solid and Liquid.Isolated solid cleans rear 120 ℃ of dry 3h with toluene, and it is to flood in the KMnO4 of 40 ℃ and toluene mixed solution that dried solid is imported temperature according to the volume ratio ratio of 1: 1, and wherein the KMnO4 mass concentration is 0.5%, and dip time is 30min.Above-mentioned material is warmed up to 150 ℃ in drying box, oven dry is to remove and to reclaim toluene.The material that obtains is carried out graphitization processing under 2300 ℃, be the product of 16～18 μ m extracting average grain diameter, material degree of graphitization 93.4%.
Comparative example 1 injects the HTHP polymeric kettle with medium temperature coal pitch 400mL, and slowly heating, heat up and temperature is remained on 430 ℃ of lower 10h under stirring condition.Also stir in coal tar with 5 times of volumes of the importing of the material after polymerization reaction.When making the temperature of this system be cooled to 290 ℃, then by centrifugal separating device with Separation of Solid and Liquid.Isolated solid cleans rear 120 ℃ of dry 3h with toluene, dried solid is carried out graphitization processing under 2800 ℃, is the product of 16～18 μ m extracting average grain diameter, material degree of graphitization 89.7%.
The quantitative measurement average grain diameter of the artificial stone tampon that makes with the present invention is measured by Britain Malvern-Mastersizer 2000 laser particle size analyzers, specific area is measured by U.S.'s health tower Qusntachrome-NOVA 1000e specific surface and porosity tester, tap density is measured by the FZS4-4 type tap density analyzer of Iron and Steel Research Geueral Inst, degree of graphitization calculates according to the crystal pitch of test and gets, and the crystal pitch of material is measured by Rigaku motor D/Max-2005X x ray diffractometer x.
Test result sees Table 1.
Table 1 physical testing result
According to the test case analysis, adopt the mixture of coal tar asphalt or coal tar asphalt and coal tar as the raw material of reaction, can reduce growth cost; Simultaneously, adopt the method for catalyzed graphitization to carry out graphitization processing under lower temperature, still can reach the degree of graphitization that does not adopt catalyzed graphitization temperature 2800 to reach.
By to making the technique adjustment of artificial graphitized mesophase phase graphite microspheres, the degree of graphitization that the conditions such as polymerization temperature, polymerization time that change can be controlled product is more than 89%, and other physical indexs are stable.
Electrochemical property test: product and oiliness binding agent PVDF (Kynoar), the conductive agent respectively above-described embodiment and comparative example made mix with the mass ratio of 90: 4: 6, binding agent PVDF should first be dissolved in NMP (1-METHYLPYRROLIDONE), the cathode size that mixes is coated on Copper Foil uniformly, and carries out drying, cut and make cathode pole piece.Positive electrode adopts LiCoO
2Be coated on aluminium foil as anode pole piece, electrolyte adopts 1.2MLiPF
6The solution of PC/EC/EMC/VC.Carry out charge-discharge test after above-mentioned material is assembled into rectangular cell, the equipment that test is used is tested as Shenzhen BTS of Xin Wei Electronics Co., Ltd. type battery test system.Test index comprises discharge capacity and first charge-discharge efficiency first, discharge voltage 4.2～2.75V.
Test result is listed in table 2.
Table 2 electrochemical property test result
By the Delanium Graphitized MCMB is carried out electric performance test, illustrate through improving the material of technique and then the manufacturing that reduces production costs, the material of more original expensive production is not all having reduction aspect physical property and chemical property, the cost of material is more than 17% simultaneously, for the cost performance that improves Graphitized MCMB, and then improve the market share of this material in lithium battery applications huge impetus is arranged.
Claims (1)
1. the preparation method of an artificial graphite cathode material for lithium ion batteries, described artificial plumbago negative pole material refers to the Graphitized MCMB synthetic take coal tar pitch as raw material, it is characterized in that comprising following process:
(1) with the mixture of coal tar pitch or coal tar pitch and coal tar, in mixture, coal tar pitch and coal tar volume ratio are 2～5: 1, add in high-temperature high-pressure reaction kettle, at 350～480 ℃, under 2～6 atmospheric pressure, thermal polymerization 5～15 hours makes the part coal tar pitch change into the mesophase pitch microballoon;
(2) the resulting mixture that contains viscoelastic phase coal tar pitch, mesophase pitch microballoon of step (1) is imported be preinstalled with in the cooling bath of this mixture room temperature coal tar of 5 times of volumes, reduce below the temperature to 300 ℃ of mixed material;
(3) step (2) gained mixture is imported centrifugation and washing in the high speed centrifugation device, the mesophase pitch microballoon is separated from other solution, and fully washed the mesophase pitch microsphere surface with solvent;
(4) the mesophase pitch microballoon that obtains with step (3) is that to be dispensed into temperature at 1: 1 be the KMnO of 40 ℃ according to volume ratio
4With flood in the toluene mixed solution, KMnO wherein
4Mass concentration is 0.1～0.5%, and dip time is 30min;
(5) then the 150 ℃ of oven dry of mixture heating that step (4) obtained contain mesophase pitch microsphere particle thing carry out graphitization processing to remove and to reclaim toluene at the temperature of 2300 ℃, obtain degree of graphitization higher than 89% Graphitized MCMB.
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| CN2009100703133A CN102005559B (en) | 2009-09-01 | 2009-09-01 | Method for preparing artificial graphite cathode material for lithium ion batteries |
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| CN103022494B (en) * | 2012-12-21 | 2013-11-06 | 济宁碳素集团有限公司 | Preparation method of synthetic graphite and application thereof |
| CN111244449B (en) * | 2018-11-28 | 2022-04-08 | 上海杉杉科技有限公司 | Modified intermediate phase negative electrode material, lithium ion secondary battery, preparation method and application |
| CN111732098A (en) * | 2020-07-01 | 2020-10-02 | 河南开炭新材料设计研究院有限公司 | Preparation method of asphalt-based carbon microspheres for lithium battery negative electrode material |
| CN113594450B (en) * | 2021-07-15 | 2023-01-13 | 山西沁新能源集团股份有限公司 | Preparation method of coal-based artificial graphite cathode material for lithium ion battery |
| CN115637329B (en) * | 2022-12-23 | 2023-03-31 | 湖南金阳烯碳新材料股份有限公司 | Recovery process of lithium ion battery negative electrode material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308113A (en) * | 2000-11-23 | 2001-08-15 | 天津大学 | Copolycondensation preparation of intermediate phase carbon microsphere |
| CN101456552A (en) * | 2009-01-06 | 2009-06-17 | 黑龙江大学 | In-situ synchronous synthesizing method of tungsten carbide/graphitic carbon nano complexes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1308113A (en) * | 2000-11-23 | 2001-08-15 | 天津大学 | Copolycondensation preparation of intermediate phase carbon microsphere |
| CN101456552A (en) * | 2009-01-06 | 2009-06-17 | 黑龙江大学 | In-situ synchronous synthesizing method of tungsten carbide/graphitic carbon nano complexes |
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